CN110092650A - High-strength light acicular mullite porous ceramics and preparation method thereof and filter - Google Patents
High-strength light acicular mullite porous ceramics and preparation method thereof and filter Download PDFInfo
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- CN110092650A CN110092650A CN201910404433.6A CN201910404433A CN110092650A CN 110092650 A CN110092650 A CN 110092650A CN 201910404433 A CN201910404433 A CN 201910404433A CN 110092650 A CN110092650 A CN 110092650A
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Abstract
The present invention provides a kind of high-strength light acicular mullite porous ceramics and preparation method thereof and filter, preparation method is the following steps are included: step S10, and by aluminium oxide, silica according to molar ratio (1.3-1.5): 1 progress ingredient obtains the first powder；Calcium carbonate, aluminium oxide, silica are subjected to ingredient according to molar ratio 1:1:2 and obtain the second powder；By first powder, the second powder and account for first powder quality 10-15% aluminum fluoride trihydrate and monomer solution be mixedly configured into slurry；The slurry is carried out foaming processing, obtains porous slurry by step S20；Step S30 makes the porous slurry that gel reaction occur, obtains green body；The green body is carried out microwave drying treatment so that the body drying by step S40；The green body after drying is sintered by step S50, obtains the high-strength light acicular mullite porous ceramics.The high-strength light acicular mullite porous ceramics long service life that the present invention obtains, intensity is high, and the porosity is high.
Description
Technical field
The present invention relates to the preparation methods of ceramic block, porous more particularly, to a kind of high-strength light acicular mullite
Ceramics and preparation method thereof, and the filter including the high-strength light acicular mullite porous ceramics.
Background technique
In recent years, with the fast development of metallurgical casting industry, the research and application of filter for molten metal receive pole
Big to pay close attention to, quantity, form, distribution, size of field trash in metallic aluminium and its alloy material etc. are to the intensity of material, plasticity
Have significant impact with toughness, therefore, research and develop practical and efficient metal purification method, with improve its comprehensive performance by
Pay attention to.And traditional refinery practice, it cannot be removed effectively tiny in melt aluminium and suspension non-metallic inclusion.Largely grind
Study carefully and show significantly remove field trash and the gas etc. in metal with ceramic filter filtering metal liquid, improves the inherence of metal
Quality.
Acicular mullite porous ceramics be exactly it is a kind of using temperature height, superhigh intensity, high porosity a kind of material, very
It is suitable as the material of filter for molten metal.However, existing technology of preparing is difficult to combine intensity and the porosity.
Summary of the invention
In view of this, the purpose of the present invention is to provide a kind of preparation sides of high-strength light acicular mullite porous ceramics
Method, can prepare while have high porosity and high-intensitive high-strength light acicular mullite porous ceramics.
Another object of the present invention is to provide a kind of while having high porosity and high-intensitive high-strength light needle-shaped not next
Stone porous ceramics, under conditions of meeting the strength of materials in the scope of application, obtain the higher porosity, more high filtration effect
The filtering material of rate, and can greatly mitigate the weight of filter, improve the effect of filtering.
Another object of the present invention is to provide a kind of lightweight, high intensity, efficient filter.
In order to solve the above technical problems, the invention adopts the following technical scheme:
The preparation method of the high-strength light acicular mullite porous ceramics of embodiment according to a first aspect of the present invention, including with
Lower step:
Step S10, by aluminium oxide, silica according to molar ratio (1.3-1.5): 1 progress ingredient obtains the first powder；It will
Calcium carbonate, aluminium oxide, silica carry out ingredient according to molar ratio 1:1:2 and obtain the second powder；Then by first powder,
Second powder and account for first powder quality 10-15% aluminum fluoride trihydrate and monomer solution be mixedly configured into slurry,
First powder is scaled mullite, second powder is scaled in anorthitic situation, described in the slurry
Mullite and the anorthitic molar ratio are (6-8): (4-2)；
The slurry is carried out foaming processing, obtains porous slurry by step S20；
Step S30 makes the porous slurry that gel reaction occur, obtains green body；
The green body is carried out microwave drying treatment so that the body drying by step S40；
The green body after drying is sintered by step S50, obtains the porous pottery of high-strength light acicular mullite
Porcelain.
Further, in the step S10, the granularity of the calcium carbonate is 600nm~800nm, the aluminium oxide
Granularity is 300nm~500nm, and the granularity of the silica is 4 μm~10 μm, and the solid content of the slurry is 20-
30vol%.
Further, the step S10 includes:
Monomer, crosslinking agent and dispersing agent are added to the water mechanical stirring to form the monomer solution by step S11；
Step S12 first powder, the second powder and aluminum fluoride trihydrate is added in the monomer solution, ball milling
15h~20h obtains the slurry,
Wherein, the monomer is acrylamide, and the crosslinking agent is N, N~methylene-bisacrylamide, the dispersing agent
For ammonium polyacrylate, the monomer is 5%~15% of the quality of water in the slurry, and the crosslinking agent is water in the slurry
Quality 0.5%~1.5%, the dispersing agent be first powder, the second powder and aluminum fluoride trihydrate gross mass
0.5%~1.5%.
Further, the step S20 is specifically included:
Foaming agent solution is added in the slurry and stirs evenly, obtains the porous slurry.Wherein, the foaming agent
Solution includes deionized water, lauryl sodium sulfate and lauryl alcohol, and lauryl sodium sulfate is the 0.1% of the quality of water, and 12
Alcohol is the 0.008% of the quality of water.Concentration of the foaming agent solution in the slurry is 1g/L~4g/L.
Further, the step S30 includes:
Catalyst is added in the porous slurry in step S31；
Step S32 is added initiator after the porous slurry is stablized and stirs evenly；
Addition is had the porous slurry of the catalyst and initiator to pour into mold so that gel occurs by step S33
Reaction obtains green body,
Wherein, in the step S31, the catalyst is tetramethylethylenediamine, and the catalyst is relative to the list
The mass ratio of body is 4%~15%；
In the step S32, the initiator is ammonium persulfate, mass ratio of the initiator relative to the monomer
It is 10%~30%.
Further, in the step S40, discontinuous microwave drying treatment is carried out to the green body, wherein when total dry
Between be 20h~40h, microwave treatment is carried out with the power of 20W~40W, the time of each microwave treatment is 5 seconds~15 seconds, twice
It is spaced 5 minutes~15 minutes between microwave treatment.
Further, the step S50 includes:
It is once sintered, the green body after drying is placed in Muffle furnace, is in the green body under sealing state respectively
In 100 DEG C, 600 DEG C of heat preservations 1h, 1200 DEG C of heat preservation 2h, in 1450 DEG C of heat preservation 5h to be sintered, cooled down with the speed of 2 DEG C/min
Furnace cooling is to room temperature after to 300 DEG C；
Once sintered body after cooling is then warming up under open state with the speed of 2 DEG C/min by double sintering
1450 DEG C of heat preservation 1h, furnace cooling to room temperature obtain the high-strength light acicular mullite porous ceramics.
The high-strength light acicular mullite porous ceramics of embodiment according to a second aspect of the present invention, according to any of the above-described institute
The preparation method for the high-strength light acicular mullite porous ceramics stated is prepared.
Further, the porosity of the high-strength light acicular mullite porous ceramics is 70%~88%, bulk density
For 0.35g/cm3~0.75g/cm3, compression strength is 1.2MPa~10.5MPa.Wherein, open porosity and bulk density use base
It is obtained in the boiling method measurement of Archimedes' principle, compression strength is surveyed by universal testing machine (WDW-100E, Changchun, China)
Fixed, specimen size is
The filter of embodiment according to a third aspect of the present invention, the carrier of the filter include according to above-described embodiment
High-strength light acicular mullite porous ceramic film material.
Above-mentioned technical proposal of the invention one of at least has the advantages that:
1) preparation method of high-strength light acicular mullite porous ceramics according to an embodiment of the present invention, obtained lightweight
High-strength acicular mullite porous ceramics purity is higher, and mullite grains are in needle-shaped cross-distribution in three-dimensional space, acicular mullite
For intercrystalline by anorthite mutually close connection, this makes high-strength light acicular mullite porous ceramics have high intensity and good
Thermal shock resistance can make when obtained high-strength light acicular mullite porous ceramic film material is used as filter
Filter has longer service life；
2) higher by using purity, the lesser raw material powder of granularity as raw material, due to its eutectic point of two phase sinterings compared with
Low, then sintering temperature is lower；And since its smaller reactivity of raw material granularity is higher, the combination degree between particle mentions significantly
Height is conducive to obtain the higher porous ceramic film material of intensity；
3) present invention combines two kinds of techniques of mechanical foaming and gel injection-moulding, prepares porous slurry using mechanical foaming technique
Expect, make porous fixed in a short time using Gel-casting process and be stabilized, greatly reduce porous rupture and polymerize, most
Uniform pore diameter and median pore size is smaller in its microstructure of the porous ceramic film material obtained eventually, the porosity is higher；
4) by using discontinuous microwave action drying process to green body, keep green body uniform from the inside to the outside in the drying process
It shrinks, reduces the generation of green body internal fissure, to improve the compression strength and thermal shock resistance of porous ceramic film material, extending it makes
Use the service life；
5) preparation method of the high-strength light acicular mullite porous ceramic film material of embodiment according to the present invention, controllability
By force, pass through object phase composition, the porosity, compression strength and the median pore size of the state modulators samples such as adjusting raw material proportioning, solid content
Distribution etc.；
6) high-strength light acicular mullite porous ceramic film material according to an embodiment of the present invention, the porosity be 70%~
88%, bulk density 0.35g/cm3~0.75g/cm3, compression strength is 1.2MPa~10.5MPa.As filter material,
Under conditions of meeting the strength of materials in the scope of application, the higher filter of the porosity is obtained, can greatly be mitigated
Quality, to improve filter effect.
Detailed description of the invention
Fig. 1 is the process according to the preparation method of the high-strength light acicular mullite porous ceramics of one embodiment of the invention
Figure；
Fig. 2 is the X-ray diffracting spectrum according to the high-strength light acicular mullite porous ceramics of the embodiment of the present invention,
In, (a) is the map of embodiment 1, (b) is the map of embodiment 2；
Fig. 3 a is the microcosmic hole of incision position according to the high-strength light acicular mullite porous ceramic film material of the embodiment of the present invention 1
The electron scanning micrograph of structure；
Fig. 3 b is the microcosmic hole of incision position according to the high-strength light acicular mullite porous ceramic film material of the embodiment of the present invention 2
The electron scanning micrograph of structure.
Specific embodiment
In order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below in conjunction with the embodiment of the present invention
Attached drawing, the technical solution of the embodiment of the present invention is clearly and completely described.Obviously, described embodiment is this hair
Bright a part of the embodiment, instead of all the embodiments.Based on described the embodiment of the present invention, ordinary skill
Personnel's every other embodiment obtained, shall fall within the protection scope of the present invention.
The preparation side of high-strength light acicular mullite porous ceramics according to an embodiment of the present invention is specifically described first below
Method.
The preparation method of high-strength light acicular mullite porous ceramic film material according to an embodiment of the present invention, as shown in Figure 1,
The following steps are included:
Step S10, by aluminium oxide, silica according to molar ratio (1.3-1.5): 1 progress ingredient obtains the first powder；It will
Calcium carbonate, aluminium oxide, silica carry out ingredient according to molar ratio 1:1:(1-2) and obtain the second powder；Then by described first
Powder, the second powder and account for first powder quality 10-15% aluminum fluoride trihydrate and monomer solution be mixedly configured into
First powder is scaled mullite, second powder is scaled in anorthitic situation, in the slurry by slurry
The mullite and the anorthitic molar ratio are (6-8): (4-2)；
The slurry is carried out foaming processing, obtains porous slurry by step S20；
Step S30 makes the porous slurry that gel reaction occur, obtains green body；
The green body is carried out microwave drying treatment so that the body drying by step S40；
The green body after drying is sintered by step S50, obtains the porous pottery of high-strength light acicular mullite
Porcelain.
In other words, some specific embodiments according to the present invention, using aluminium oxide, silica, calcium carbonate and three water fluorine
Changing aluminium is that raw material prepares high-strength light acicular mullite porous ceramic film material, firstly, to prepare mullite for aluminium oxide: silica
With molar ratio for (1.3-1.5): 1 is matched to obtain the first powder, to prepare anorthite for calcium carbonate: aluminium oxide: silica
It is that 1:1:2 progress ingredient obtains the second powder, then aluminum fluoride trihydrate is added by the 12% of mullite quality with molar ratio, then will
Ingredient is according to mullite: anorthitic molar ratio (6-8): (4-2) and water are mixedly configured into slurry, then, attached gel injection molding
Molding and mechanical stirring foam process prepare porous ceramics green body using the porous method of coagulating of infusing, i.e., foaming are added in mixed slurry
Agent simultaneously obtains porous slurry by mechanical stirring, then porous slurry is poured into mold to bring it about gel reaction, acquires
Green body, finally, using microwave drying process, then the green body after drying is placed in sintering furnace and is sintered, obtain high-strength light
Acicular mullite porous ceramic film material.Herein, it is to be understood that due to using aluminum fluoride trihydrate to introduce a certain amount of aluminium, because
This can suitably reduce the proportion of aluminium component when being equipped with and being intended to prepare the first powder of mullite.
The preparation method of high-strength light acicular mullite porous ceramics according to an embodiment of the present invention as a result, due to stringent
Ingredient, obtained high-strength light acicular mullite porous ceramic film material are carried out according to the proportion of high-strength light acicular mullite phase
Purity is higher, is tightly combined in high-strength light acicular mullite porous ceramic film material, and integral strength improves.In addition, passing through adjusting
The ratio (in other words, passing through the amount of mullite crystal whisker in adjusting target product) of first powder and the second powder, can control sample
The porosity, compression strength and specific gravity of product etc..
The microstructure of porous material is extremely complex, and when the temperature increases, the process of phonon transmitting is hindered, complicated
Stomata, acicular mullite grains and tiny anorthite crystal grain therebetween scatter lattice wave, anorthite and mullite
Similar thermal expansion coefficient, i.e. high-strength light acicular mullite porous material have high intensity and good thermal shock resistance, when
When obtained high-strength light acicular mullite porous ceramic film material is used as filter, filter can be made to have longer make
Use the service life.
In addition, the present invention combines two kinds of techniques of mechanical foaming and gel injection-moulding, prepared using mechanical foaming technique more
Hole slurry makes porous fixed in a short time and is stabilized, greatly reduces porous rupture and gathers using Gel-casting process
It closes, uniform pore diameter and median pore size is smaller in its microstructure of finally obtained porous ceramic film material, specific surface area is bigger.According to
The high-strength light acicular mullite that the preparation method of the high-strength light acicular mullite porous ceramics of the embodiment of the present invention obtains is more
The porosity of hole ceramics is 70%~88%, bulk density 0.35g/cm3~0.75g/cm3, compression strength be 1.2MPa~
10.5MPa.High-strength light acicular mullite porous ceramic film material according to an embodiment of the present invention has intensity high and porosity height
The characteristics of, there is higher intensity with filter prepared by the high-strength light acicular mullite porous ceramic film material, filter
Service life is greatly improved, and application range is wider.
According to one embodiment of present invention, in step slo, ingredient is that purity is higher, the lesser raw material powder of granularity,
In, the granularity 800nm of the calcium carbonate, the granularity of the aluminium oxide is 300nm~500nm, and the granularity of the silica is 4
μm~solid content of 10 μm and the slurry is 20-30vol%.Due to there is sintering aid in raw material, eutectic point is lower, therefore is not required to
Higher sintering temperature is wanted, green body is still able to maintain porous structure at a relatively low sintering temperature, but has after sintering a small amount of
Impurity phase, further, since the granularity of ingredient is smaller, reactivity is higher, and the combination degree between particle is high, is conducive to obtain strong
Spend higher porous ceramic film material.In addition, being conducive to the intensity for controlling green body by adjusting solid concentration, and then control final
The intensity of ceramic body.
According to one embodiment of present invention, step S10 includes:
Monomer, crosslinking agent and dispersing agent are added to the water mechanical stirring to form the monomer solution by step S11；
Step S12 first powder, the second powder and aluminum fluoride trihydrate is added in the monomer solution, ball milling
15h~20h obtains the slurry,
Wherein, the monomer is acrylamide, and the crosslinking agent is N, N~methylene-bisacrylamide, the dispersing agent
For ammonium polyacrylate, the monomer is 5%~15% of the quality of water in the slurry, and the crosslinking agent is water in the slurry
Quality 0.5%~1.5%, the dispersing agent be first powder, the second powder and aluminum fluoride trihydrate gross mass
0.5%~1.5%.
According to one embodiment of present invention, step S20 is specifically included:
Foaming agent solution is added in the slurry and stirs evenly, obtains the porous slurry.
Wherein, the foaming agent solution includes deionized water, lauryl sodium sulfate and lauryl alcohol, lauryl sodium sulfate
It is the 0.1% of the quality of water, lauryl alcohol is the 0.008% of the quality of water.Concentration of the foaming agent solution in the slurry
For 1g/L~4g/L.Foam volume is adjusted by adjusting the content of foaming agent, facilitates the porosity, the pressure resistance that control sample
Degree and median pore size distribution etc..
Further, the step S30 may include:
Catalyst is added in the porous slurry in step S31；
Step S32 is added initiator after the porous slurry is stablized and stirs evenly；
Addition is had the porous slurry of the catalyst and initiator to pour into mold so that gel occurs by step S33
Reaction obtains green body,
Wherein, in the step S31, the catalyst is tetramethylethylenediamine, and the catalyst is relative to the list
The mass ratio of body is 4%~15%；
In the step S32, the initiator is ammonium persulfate, mass ratio of the initiator relative to the monomer
It is 10%~30%.That is, firstly, foaming agent (lauryl sodium sulfate) being added in porous slurry and carries out machinery and stirs
It mixes, obtains uniform and stable porous slurry, then, porous slurry is poured into mold to bring it about gel reaction to acquire
Green body, then catalyst (tetramethylethylenediamine) is added into porous slurry, initiator (ammonium persulfate) is added after slurry is stablized
And poured into mold after being sufficiently stirred, gel reaction occurs under the action of catalyst and initiator for monomer and crosslinking agent same at this time
When release heat, demoulded after the gel reaction of monomer, obtain green body.
The preparation method of high-strength light acicular mullite porous ceramic film material according to an embodiment of the present invention as a result, by machine
Tool foaming and two kinds of techniques of gel injection-moulding combine, and prepare porous slurry using mechanical foaming technique, utilize Gel-casting process
Make porous fixation in a short time and is stabilized, greatly reduces porous rupture and polymerize, finally obtained porous ceramics material
Expect uniform pore diameter in its microstructure and median pore size is smaller, the porosity is higher.
According to one embodiment of present invention, in step S40, discontinuous microwave drying treatment is carried out to green body, wherein total
Drying time is 20h~40h, carries out microwave treatment with the power of 20W~40W, the time of each microwave treatment is 5 seconds~15
Second, it is spaced 5 minutes~15 minutes between microwave treatment twice.By using discontinuous microwave action drying process to green body, make
Green body uniform shrinkage from the inside to the outside in the drying process, reduces the generation of green body internal fissure, to improve porous ceramic film material
Compression strength and thermal shock resistance, prolong its service life.
According to one embodiment of present invention, step S50 includes:
It is once sintered, the green body after drying is placed in Muffle furnace in sealed states respectively at 100 DEG C, 600 DEG C
Heat preservation 1h, 1200 DEG C of heat preservation 2h are cooled to after 300 DEG C with the speed of 2 DEG C/min with furnace in 1450 DEG C of heat preservation 5h to be sintered
It is cooled to room temperature；
Once sintered body after cooling is then warming up under open state with the speed of 2 DEG C/min by double sintering
1450 DEG C of heat preservation 1h, furnace cooling to room temperature.
In once sintered, it is completely dried it by the way that green body is kept the temperature 1 hour at 100 DEG C, then by by green body
It keeps the temperature 1 hour at 600 DEG C and makes gel to exclude by cracking, hereafter calcium carbonate reaction of decomposing generates calcium oxide and then generates
Anorthite nucleus, mullite crystal whisker forming core finally make mullite crystal whisker grow up and mullite grains in 1450 DEG C of high temperature sinterings
In needle-shaped cross-distribution by anorthite mutually close connection between three-dimensional space, acicular mullite grains；Due to it is once sintered be place
(in laboratory experiment, green body is placed in crucible, and crucible capping is sintered) in sealing state, therefore colloid cracks
The carbon of generation cannot exclude completely, cause porous ceramics generated in black.For this purpose, once sintered body after cooling is being opened
It puts to be sintered again under state and carries out row's carbon, while anorthite is further grown up and improves the intensity of the porous ceramics.
The lightweight that the preparation method of high-strength light acicular mullite porous ceramic film material according to an embodiment of the present invention obtains
High-strength acicular mullite porous ceramic film material, the porosity are 70%~88%, bulk density 0.35g/cm3~0.75g/cm3,
Compression strength is 1.2MPa~10.5MPa, as filter material, under conditions of meeting the strength of materials in the scope of application,
The higher filter of the porosity is obtained, it can be greatly by mitigating the quality of filter, to mitigate the quality of filter.
The system of high-strength light acicular mullite porous ceramic film material according to the present invention is described combined with specific embodiments below
Preparation Method.
It should be noted that, using acrylamide as monomer, N, N~methylene-bisacrylamide is to hand in following embodiments
Join agent, tetramethylethylenediamine is catalyst, and ammonium persulfate is is illustrated for the gelation reaction for initiator, but sheet
Invention is not limited to this, can also be using the gelation reaction of other any reagents known to those skilled in the art.In addition, following realities
It applies in example and is illustrated by foaming agent of lauryl sodium sulfate, but the present invention is not limited thereto, those skilled in the art can adopt
Foaming processing is carried out with any other foaming agents.Scheme after these changes, all should be understood that and belongs to guarantor of the invention
It protects in range.
Embodiment 1
Firstly, respectively by acrylamide (monomer), N, N~methylene-bisacrylamide (crosslinking agent) according to water quality
10wt% and 1wt% are added to the water, and add the ammonium polyacrylate (dispersing agent) of raw ceramic materials powder gross mass 0.5wt%, mixing
Uniformly obtain monomer solution.
Prepare ceramic powder, wherein calcium carbonate (granularity 600nm), aluminium oxide (granularity 350nm), silica (grain
Degree is 10 μm) and aluminum fluoride trihydrate (analysis is pure), so that ceramic powder, relative to above-mentioned monomer solution, solid content control exists
25vol%.
Wherein, it is matched to obtain the first powder with the aluminium oxide of 1.33:1 molar ratio and silica, it is intended to fabricated in situ
Mullite；Calcium carbonate, aluminium oxide and silica with molar ratio for 1:1:2 are matched to obtain the first powder, it is intended to are used for
Synthesize anorthite；And calculated respectively with anorthite and mullite, so that the dosage of the first powder and the second powder meets calcium
The molar ratio of feldspar and mullite is 2:8.And the dosage of aluminum fluoride trihydrate is the mass ratio 12% of the first powder, for promoting not
Carry out the generation of stone crystal whisker.
Load weighted ceramic powder is placed in ball grinder together with monomer solution and is placed on tumbling ball mill and is mixed
18h。
Secondly, mixed slurry is poured out, the foaming agent solution that 1g/L is added in the slurry foams, and stirs 10min
After make foam volume stablize at 4 times.Wherein, foaming agent solution includes deionized water, lauryl sodium sulfate and lauryl alcohol, and 12
Sodium alkyl sulfate is the 0.1% of the quality of water, and lauryl alcohol is the 0.008% of the quality of water.The foaming agent solution is in the slurry
Concentration in material is 1g/L~4g/L.
Then, the tetramethylethylenediamine (catalyst) of acrylamide quality 11.25% is added, propylene is added after stirring 5min
The ammonium persulfate (initiator) of amide quality 25% continues directly to pour into slurry in disposable tool after stirring 3min, stand
Find that outer mold wall obviously generates heat after 3min, at this time acrylamide and N, N~methylene-bisacrylamide is in tetramethylethylenediamine
With polymerization reaction occurs under the action of ammonium persulfate, after outer mold wall temperature is reduced to room temperature carry out damage type demoulding.
Next, the green body after demoulding is placed in microwave drying oven dry 30h, operating power 30W, at each microwave
The action time of reason is 10s, and the interval time between microwave treatment is 10min twice.
Calcining is sintered finally, the green body after drying is placed in Muffle furnace: being in the green body under sealing state
It is once sintered in 1450 DEG C of heat preservation 5h progress respectively in 100 DEG C, 600 DEG C of heat preservations 1h, 1200 DEG C of heat preservation 2h, hereafter with 2 DEG C/min
Speed cool to 300 DEG C after furnace cooling to room temperature, finally by once sintered body after cooling under open state with 2 DEG C/
1450 DEG C of heat preservation 1h of speed heating of min carry out double sinterings, and it is more to obtain high-strength light acicular mullite for furnace cooling to room temperature
Hole ceramics.
X-ray diffraction (XRD) map of the high-strength acicular mullite ceramic material powder of the porous light obtained as a result, is such as
In Fig. 2 shown in (a), (a) is as can be seen that the material is mainly mullite and a small amount of anorthite from Fig. 2.High-strength light is needle-shaped
The microstructural electron scanning micrograph of mullite porous ceramic section is as shown in Figure 3a, it is seen that material air hole structure is equal
Even, acicular mullite crystal development is good, and the length of acicular mullite crystal is at 200 μm or so.Gained high-strength light is needle-shaped not
The porosity for carrying out stone porous ceramic film material is 87.55%, bulk density 0.4g/cm3, compression strength 2.08MPa.Wherein,
Open porosity and bulk density are obtained using the boiling method measurement based on Archimedes' principle, and compression strength passes through universal testing machine
(WDW-100E, Changchun, China) measurement, specimen size are
Embodiment 2
Firstly, respectively by acrylamide (monomer), N, N~methylene-bisacrylamide (crosslinking agent) according to water quality
10wt% and 1wt% are added to the water, and add the ammonium polyacrylate (dispersing agent) of raw ceramic materials powder gross mass 0.5wt%, mixing
Uniformly obtain premixed liquid.
Prepare ceramic powder, wherein calcium carbonate (granularity 800nm), aluminium oxide (granularity 450nm), silica (grain
Degree is 10 μm) and aluminum fluoride trihydrate (analysis is pure), so that ceramic powder, relative to above-mentioned monomer solution, solid content control exists
25vol%.
Wherein, it is matched to obtain the first powder with the aluminium oxide of 1.4:1 molar ratio and silica, it is intended to which fabricated in situ is not
Carry out stone；Calcium carbonate, aluminium oxide and silica with molar ratio for 1:1:2 are matched to obtain the first powder, it is intended to for closing
At anorthite；And calculated respectively with anorthite and mullite, so as to meet calcium long for the dosage of the first powder and the second powder
The molar ratio of stone and mullite is 4:6.And the dosage of aluminum fluoride trihydrate is the mass ratio 12% of the first powder, for promoting not come
The generation of stone crystal whisker.
Load weighted ceramic powder is placed in ball grinder together with monomer solution and is placed on tumbling ball mill and is mixed
18h。
Then, foamed, gel casting, microwave drying and sintering, each process flow reference implementation example 1.
X-ray diffraction (XRD) map of the high-strength acicular mullite ceramic material powder of the porous light obtained as a result, is such as
In Fig. 2 shown in (b), (b) has a small amount of aluminium oxide to deposit as can be seen that the material is mainly mullite and anorthite from Fig. 2
?.The microstructural electron scanning micrograph of high-strength light acicular mullite porous ceramics section is as shown in Figure 3b, it is seen that
The ball-type air hole structure of material remains intact, and acicular mullite crystal development is good, mutually overlaps between whisker, calcium on hole wall
Feldspar and acicular mullite crystal combination are close.The porosity of gained high-strength light acicular mullite porous ceramic film material is
85.77%, bulk density 0.42g/cm3, compression strength 11.24MPa.
It is better than the performance of existing filter according to the performance data that this experiment of literature survey obtains.According to aforementioned present invention
The high-strength light acicular mullite porous ceramic film material of embodiment is significantly larger than existing requirement, can be adapted for completely porous
Ceramic filter.
In addition, known to comprehensive four examples and laboratory abundant experimental results: as mullite contains under identical sintering temperature
The porosity of the increase of amount, material increases, but strength reduction；As sintering temperature increases, porosity decline, but intensity increases.
It can be expired by rationally designing object Phase Proportion, sintering temperature and sintering schedule, the available porosity and intensity
The high-strength light acicular mullite porous ceramics product of sufficient application requirement.
Compared to this, according to reports, the technical parameter requirement that Wei's army et al. summarizes existing filter for molten metal is as follows,
0.8~1.5MPa of compression strength, porosity of=80%, 0.3~1g/cm of bulk density3, use temperature >=1200 DEG C.And according to
High-strength light acicular mullite porous ceramic film material prepared by the present invention can achieve identical even higher performance, have wide
Applicable prospect.
The above is a preferred embodiment of the present invention, it is noted that for those skilled in the art
For, without departing from the principles of the present invention, several improvements and modifications can also be made, these improvements and modifications
It should be regarded as protection scope of the present invention.
Claims (10)
1. a kind of preparation method of high-strength light acicular mullite porous ceramics, which comprises the following steps:
Step S10, by aluminium oxide, silica according to molar ratio (1.3-1.5): 1 progress ingredient obtains the first powder；By carbonic acid
Calcium, aluminium oxide, silica carry out ingredient according to molar ratio 1:1:2 and obtain the second powder；By first powder, the second powder
And account for the aluminum fluoride trihydrate of the 10-15% of first powder quality and monomer solution is mixedly configured into slurry, by described the
One powder is scaled mullite, and second powder is scaled in anorthitic situation, mullite described in the slurry with
The anorthitic molar ratio is (6-8): (4-2)；
The slurry is carried out foaming processing, obtains porous slurry by step S20；
Step S30 makes the porous slurry that gel reaction occur, obtains green body；
The green body is carried out microwave drying treatment so that the body drying by step S40；
The green body after drying is sintered by step S50, obtains the high-strength light acicular mullite porous ceramics.
2. the preparation method of high-strength light acicular mullite porous ceramics according to claim 1, which is characterized in that in institute
It states in step S10, the granularity of the calcium carbonate is 600-800nm, and the granularity of the aluminium oxide is 300nm~500nm, described two
The granularity of silica is 4 μm~10 μm, and the solid content of the slurry is 20-30vol%.
3. the preparation method of high-strength light acicular mullite porous ceramics according to claim 1, which is characterized in that described
Step S10 includes:
Monomer, crosslinking agent and dispersing agent are added to the water mechanical stirring to form the monomer solution by step S11；
First powder, the second powder and aluminum fluoride trihydrate are added in the monomer solution step S12, and ball milling 15h~
20h obtains the slurry,
Wherein, the monomer is acrylamide, and the crosslinking agent is N, and N~methylene-bisacrylamide, the dispersing agent is poly-
Ammonium acrylate, the monomer are 5%~15% of the quality of water in the slurry, and the crosslinking agent is the matter of water in the slurry
The 0.5%~1.5% of amount, the dispersing agent are the gross mass of first powder, the second powder and aluminum fluoride trihydrate
0.5%~1.5%.
4. the preparation method of high-strength light acicular mullite porous ceramics according to claim 1, which is characterized in that described
Step S20 is specifically included:
Foaming agent solution is added in the slurry and stirs evenly, obtains the porous slurry,
Wherein, the foaming agent solution includes deionized water, lauryl sodium sulfate and lauryl alcohol, and lauryl sodium sulfate is water
Quality 0.1%, lauryl alcohol be water quality 0.008%,
Content of the foaming agent solution in the slurry is 1g/L~4g/L.
5. the preparation method of high-strength light acicular mullite porous ceramics according to claim 3, which is characterized in that described
Step S30 includes:
Catalyst is added in the porous slurry in step S31；
Step S32 is added initiator after the porous slurry is stablized and stirs evenly；
Addition is had the porous slurry of the catalyst and initiator to pour into gel reaction occurs in mold by step S33,
Green body is obtained,
Wherein, in the step S31, the catalyst is tetramethylethylenediamine, and the catalyst is relative to the monomer
Mass ratio is 4%~15%；
In the step S32, the initiator is ammonium persulfate, and the initiator is relative to the mass ratio of the monomer
10%~30%.
6. the preparation method of high-strength light acicular mullite porous ceramics according to claim 1, which is characterized in that in institute
State step S40, discontinuous microwave drying treatment carried out to the green body, wherein total drying time is 20h~40h, with 20W~
The power of 40W carries out microwave treatment, and the time of each microwave treatment is 5 seconds~15 seconds, is spaced 5 minutes between microwave treatment twice
~15 minutes.
7. the preparation method of acicular mullite porous ceramics according to claim 1, which is characterized in that in the step
S50 includes:
It is once sintered, the green body after drying is placed in Muffle furnace, is in the green body under sealing state respectively 100
DEG C, 600 DEG C of heat preservations 1h, 1200 DEG C of heat preservation 2h in 1450 DEG C of heat preservation 5h to be sintered cool to 300 with the speed of 2 DEG C/min
Furnace cooling is to room temperature after DEG C；
Once sintered body after cooling is then warming up to 1450 DEG C under open state with the speed of 2 DEG C/min by double sintering
1h is kept the temperature, furnace cooling to room temperature obtains the high-strength light acicular mullite porous ceramics.
8. a kind of high-strength light acicular mullite porous ceramics, which is characterized in that according to any one of claims 1 to 7
The preparation method of high-strength light acicular mullite porous ceramics is prepared.
9. high-strength light acicular mullite porous ceramics according to claim 8, which is characterized in that the high-strength light needle
The porosity of shape mullite porous ceramic is 70%~88%, bulk density 0.35g/cm3~0.75g/cm3, compression strength is
1.2MPa~10.5MPa.
10. a kind of filter, which is characterized in that the filter includes that high-strength light according to claim 1 is needle-shaped not
Carry out stone porous ceramics.
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